Proton NMR acquisition and processing conditions - DOC by COi98Y

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									Typical parameters used to record 1H 13C HMQC NMR spectra on
the DPX-400, Avance-400 and Avance-500.


DPX-400 (Old-400 in F114a)
2D gradient-enhanced HMQC 1H-13C NMR spectra were obtained on a Bruker DPX-
400 MHz spectrometer operating at 400.13 MHz for protons and 100.61 MHz for
carbon, employing a high-resolution dual(1H 13C) gradients probe. The hmqcgpqf
pulse program was used with P90 = 11.8 μs, 1JCH coupling of 145Hz, waltz decoupling
of the 13C channel was applied during acquisition, spectra were typically recorded
over an automatically optimised sweep-width with 2k data points in the f2 domain and
128 experiments in the f1 domain, FID’s were modified with a Qsine function (2) and
linear prediction used to enhance the f1 domain, data were Fourier transformed using
4k data points f2 domain and 1k data points in the f1 domain.

Avanve-400 ultra shield (New-400 in F113)
2D gradient-enhanced HMQC 1H-13C NMR spectra were obtained on a Bruker ultra-
shield Avance-400 MHz spectrometer operating at 400.13 MHz for protons and
100.61 MHz for carbon, employing a high-resolution broad-band ATMA gradients
probe. The hmqcgpqf pulse program was used with P90 = 15.25 μs, 1JCH coupling of
145Hz, waltz decoupling of the 13C channel was applied during acquisition, spectra
were typically recorded over an automatically optimised sweep-width with 2k data
points in the f2 domain and 128 experiments in the f1 domain, FID’s were modified
with a Qsine function (2) and linear prediction used to enhance the f1 domain, data
were Fourier transformed using 4k data points f2 domain and 1k data points in the f1
domain.

Avanve-500 (In F202)
2D HMQC 1H-13C NMR spectra were obtained on a Bruker Avance 500 MHz
spectrometer operating at 500.13 MHz for protons and 125.61 MHz for carbon,
employing a high-resolution 5mm broad-band HX probe. The inverse hmqcbiqf pulse
program was used with a normal geometry coil arrangement allowing hetero-nuclear
correlation to be achieved by zero quantum and double quantum coherence, cleaned
using a BIRD sequence and with decoupling during acquisition. A P90 of 12.5 μs was
used with a GARP sequence using power of 20 dB and P90 of 80 μs. Spectra were
typically recorded with 2K data points in the f2 domain and 250 ppm and 256
experiments in the f1 domain, FID’s were modified with a sin function (2) and linear
prediction used to enhance the f1 domain, data were Fourier transformed using 4k data
points f2 domain and 1k data points in the f1 domain.

								
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